CN105296771B - A kind of method using ilmenite concentrate production rich-titanium material - Google Patents
A kind of method using ilmenite concentrate production rich-titanium material Download PDFInfo
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- CN105296771B CN105296771B CN201510813700.7A CN201510813700A CN105296771B CN 105296771 B CN105296771 B CN 105296771B CN 201510813700 A CN201510813700 A CN 201510813700A CN 105296771 B CN105296771 B CN 105296771B
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Abstract
A kind of method using ilmenite concentrate production rich-titanium material comprises the following steps：Leaching centrifuges, crystallisation by cooling.The beneficial effects of the invention are as follows：（1）Present invention process process is simple, and device therefor is common device, and low energy consumption for rich-titanium material preparation process, and products obtained therefrom quality is high.（2）Prepared by traditional ilmenite can generate a large amount of pollutions during rich-titanium material, and leaching agent used in the present invention has the characteristics that environmentally friendly, nontoxic, and leaching process is more green.（3）Traditional leaching process leaching agent removal process is complicated, and the i.e. recyclable excessive leaching agent of crystallisation by cooling is only needed in the present invention, and removal process is simpler efficiently.（4）Reagent during traditional ilmenite preparation rich-titanium material can react with titanium component, the rate of recovery for causing titanium component is relatively low, and under conditions of described in the present invention, leaching agent does not react with the titanium component in ilmenite, thus, heretofore described method titanium component rate higher.
Description
Technical field
The invention belongs to metallurgical and chemical fields, are related to a kind of method using ilmenite concentrate production rich-titanium material.
Background technology
Ilmenite is the natural oxidation ore of titanium, also known as titanomagnetite, is important Ti industry raw material.The natural ore deposit of common titanium
Object has rutile and ilmenite etc., natural rutile resource TiO2Content is higher, generally only needs rear TiO during gravity separation2Contain
Amount can reach 90% or so, and then directly as Ti industry raw material.And the content of natural ferrotianium ore resources titanium component is relatively low,
Ore dressing process, which need to be passed through, can just obtain ilmenite concentrate, TiO in ilmenite after ore dressing2Content is about 46% or so.
TiO in the concentrate of ilmenite2Content still reaches to the requirement less than preferable Ti industry raw material, preferable Ti industry raw material
Usually require that TiO2Content reaches more than 85%.Thus, ilmenite concentrate, which still needs to be further processed, can be only achieved preferable Ti industry original
The requirement of material.The approach of ilmenite preparation rich-titanium material, which sums up, can be divided into two classes, and the first kind is prepared by reduction-magnetic selection method
Rich-titanium material.This kind of method is to mix ilmenite concentrate with reducing agent, is heated under the high temperature conditions, under the high temperature conditions, ferrotianium
Ferriferous oxide in ore deposit is reduced into metallic iron, crushes material after cooling, is ground to certain particle size, and magnetic separation obtains metallic iron
And titanium slag.Second class method is to remove various impurity after the titanium component in ilmenite is leached with the concentrated sulfuric acid or concentrated hydrochloric acid etc., most
Rich-titanium material is obtained eventually.Rich-titanium material is prepared by both the above approach, all there are the problems such as corresponding environment and high energy consumption.Thus,
It is the problem that rich-titanium material production field is extremely paid close attention to using cleaning and energy saving method production rich-titanium material.
The content of the invention
The problems such as in order to avoid the environmental pollution in existing rich-titanium material production process and higher energy consumption, the present invention is intended to provide
A kind of clean method that rich-titanium material is prepared using ilmenite as raw material.Compared to traditional handicraft, this method more energy conservation and environmental protection leaches
Agent is nontoxic, recyclable, can finally prepare the rich-titanium material product of high-quality.
Technical scheme mainly includes the following steps：
（1）By ilmenite concentrate as in Ball-stirring mill, leaching agent is configured to the solution that concentration is 2.5% ~ 30% with water, then
Solution is leached into 5-10 as in Ball-stirring mill, the weight ratio of ilmenite concentrate and leaching agent is stirred at room temperature for 1 than 0.1-2.5
Hour；
（2）By the material filtering after leaching, filter cake and filtrate are obtained, filtrate is carried out according to the solubility curve of leaching agent
It is fully cooled, excessive leaching agent is made to crystallize into crystal in filtrate, is filtered again after crystallization, you can recycle excessive leaching
Agent.
（3）Filter cake is pressed into filter cake：Water=1:1 ~ 4 mass ratio adds in water, obtains slurry, slurry is centrifuged, and centrifuges
After, rich-titanium material density is larger and color is black, and positioned at lower floor, remaining material density is smaller and color is grey, is located at
Upper strata is separated positioned at by the upper and lower, and lower floor is rich-titanium material.
Step（1）Described in ilmenite concentrate granularity be less than 200 μm, further, the granularity of ilmenite concentrate is in
Between 100 ~ 200 μm.Meanwhile step（1）Described in Ball-stirring mill use non-metallic material stirrer paddle and agitated medium, into
One step, stirring slurry use polytetrafluoroethylene (PTFE) material, and agitated medium uses the ball of planetary native oxide material.Step（1）In
Organic acid is used as leaching agent, further, step（1）In leaching agent for oxalic acid or citric acid, more further, step（1）In
Leaching agent be citric acid.
Step（2）In extraction temperature be room temperature to 100 DEG C, further, step（2）In extraction temperature for 50 DEG C extremely
100 DEG C, particularly preferably, step（2）In extraction temperature be 75 DEG C.Step（2）Described in Ball-stirring mill rotating speed for 10 ~
100 revs/min, further, the rotating speed of Ball-stirring mill is 50 ~ 100 revs/min, particularly preferably, the rotating speed of Ball-stirring mill for 60 turns/
Minute.Step（2）When the time of middle leaching is 5-10 small, further, when the time of leaching is 7.5-10 small, particularly preferably
Ground, when the time of leaching is 8 small.
Step（3）Described in centrifuge speed for 100 ~ 3000 revs/min, further, step（3）Described in centrifugation
Machine rotating speed is 1000 ~ 3000 revs/min, particularly preferably, centrifuge speed is 1500 revs/min, and it is not low to centrifuge the time
In 20 minutes.
TiO in the rich-titanium material2Mass percentage be more than 90%, the rate of recovery be higher than 80%.
Compared with prior art, the beneficial effects of the invention are as follows：
（1）Present invention process process is simple, and device therefor is common device, and low energy consumption for rich-titanium material preparation process, gained
Product quality is high.
（2）Traditional ilmenite can generate a large amount of pollutions during preparing rich-titanium material, and leaching agent has ring used in the present invention
The characteristics of protecting, is nontoxic, leaching process is more green.
（3）Traditional leaching process leaching agent removal process is complicated, and the i.e. recyclable excess of crystallisation by cooling is only needed in the present invention
Leaching agent, removal process it is simpler efficiently.
（4）Reagent during traditional ilmenite preparation rich-titanium material can react with titanium component, cause returning for titanium component
Yield is relatively low, and under conditions of described in the present invention, leaching agent does not react with the titanium component in ilmenite, thus, this hair
Method titanium component rate higher described in bright.
Description of the drawings
Fig. 1 is the method for the present invention flow chart.
Specific embodiment：
With reference to specific example, the present invention will be further described.
Embodiment 1
It takes 2kg ilmenite concentrates, between granularity is 120 ~ 200 μm, is put in Ball-stirring mill, weighs 1kg citric acids in room temperature
Under be configured to solution, solution is poured into Ball-stirring mill, open Ball-stirring mill, rotating speed be 30 revs/min, leaching 6 is stirred at room temperature
Hour, stop stirring, filtering by filtrate crystallisation by cooling, recycles Citric acid crystal.Filter cake is pressed into filter cake：Water=1:1.2 matter
Amount ratio adds in water, and the mixture of filter cake and water is put into centrifuge, opens centrifuge, and setting speed is 1000 revs/min, from
The heart stops after twenty minutes, and after centrifugation, rich-titanium material density is larger and color is black, positioned at lower floor, remaining material density compared with
Small and color is grey, and positioned at upper strata, the upper and lower are separated, and lower floor is rich-titanium material, measures TiO in rich-titanium material2Content
For 90.5%, the rate of recovery 80.03% of titanium.
Embodiment 2
It takes 1kg ilmenite concentrates, between granularity is 150 ~ 200 μm, is put in Ball-stirring mill, weighs 800g citric acids in room temperature
Under be configured to solution, solution is poured into Ball-stirring mill, open Ball-stirring mill, rotating speed be 40 revs/min, leaching is stirred at room temperature
5.5 it is small when, stop stirring, filtering by filtrate crystallisation by cooling, recycles Citric acid crystal.Filter cake is pressed into filter cake：Water=1:1.4
Mass ratio adds in water, and the mixture of filter cake and water is put into centrifuge, opens centrifuge, and setting speed is 1200 revs/min,
Centrifugation stops after 25 minutes, and after centrifugation, rich-titanium material density is larger and color is black, positioned at lower floor, remaining material density
Smaller and color is grey, and positioned at upper strata, the upper and lower are separated, and lower floor is rich-titanium material, measures TiO in rich-titanium material2Contain
It measures as 91.7%, the rate of recovery 80.17% of titanium.
Embodiment 3
It takes 500g ilmenite concentrates, between granularity is 100 ~ 150 μm, is put in Ball-stirring mill, weighs 500g citric acids in room
Solution is configured under temperature, solution is poured into Ball-stirring mill, opens Ball-stirring mill, rotating speed is 45 revs/min, and leaching is stirred at room temperature
7.5 it is small when, stop stirring, filtering by filtrate crystallisation by cooling, recycles Citric acid crystal.Filter cake is pressed into filter cake：Water=1:1.2
Mass ratio adds in water, and the mixture of filter cake and water is put into centrifuge, opens centrifuge, and setting speed is 1500 revs/min,
Centrifugation stops after 25 minutes, and after centrifugation, rich-titanium material density is larger and color is black, positioned at lower floor, remaining material density
Smaller and color is grey, and positioned at upper strata, the upper and lower are separated, and lower floor is rich-titanium material, measures TiO in rich-titanium material2Contain
It measures as 90.35%, 81.20 % of the rate of recovery of titanium.
Embodiment 4
It takes 200g ilmenite concentrates, between granularity is 120 ~ 180 μm, is put in Ball-stirring mill, weighs 500g citric acids 50
Solution is configured at DEG C, solution is poured into Ball-stirring mill, opens Ball-stirring mill, rotating speed is 60 revs/min, the leaching at 50 DEG C
5.5 it is small when, stop stirring, filtering by filtrate crystallisation by cooling, recycles Citric acid crystal.Filter cake is pressed into filter cake：Water=1:1.5
Mass ratio adds in water, and the mixture of filter cake and water is put into centrifuge, opens centrifuge, and setting speed is 1500 revs/min,
Centrifugation stops after twenty minutes, and after centrifugation, rich-titanium material density is larger and color is black, positioned at lower floor, remaining material density
Smaller and color is grey, and positioned at upper strata, the upper and lower are separated, and lower floor is rich-titanium material, measures TiO in rich-titanium material2Contain
It measures as 90.83%, the rate of recovery 80.33% of titanium.
Embodiment 5
It takes 250g ilmenite concentrates, between granularity is 74 ~ 150 μm, is put in Ball-stirring mill, weighs 250g citric acids at 75 DEG C
Under be configured to solution, solution is poured into Ball-stirring mill, open Ball-stirring mill, rotating speed be 60 revs/min, the leaching at 75 DEG C
8.5 it is small when, stop stirring, filtering by filtrate crystallisation by cooling, recycles Citric acid crystal.Filter cake is pressed into filter cake：Water=1:2 matter
Amount ratio adds in water, and the mixture of filter cake and water is put into centrifuge, opens centrifuge, and setting speed is 1700 revs/min, from
The heart stops after twenty minutes, and after centrifugation, rich-titanium material density is larger and color is black, positioned at lower floor, remaining material density compared with
Small and color is grey, and positioned at upper strata, the upper and lower are separated, and lower floor is rich-titanium material, measures TiO in rich-titanium material2Content
For 91.27%, the rate of recovery 80.28% of titanium.
Embodiment 6
It takes 350g ilmenite concentrates, between granularity is 150 ~ 200 μm, is put in Ball-stirring mill, weighs 250g citric acids and grass
Acid blend（100 grams of oxalic acid, 150 grams of citric acid）, solution is configured at 75 DEG C, solution is poured into Ball-stirring mill, opening is stirred
Mill is mixed, rotating speed is 75 revs/min, when leaching 8.5 is small at 75 DEG C, stops stirring, filtering by filtrate crystallisation by cooling, is returned
Receive Citric acid crystal.Filter cake is pressed into filter cake：Water=1:2.5 mass ratio adds in water, and the mixture of filter cake and water is put into centrifugation
In machine, centrifuge is opened, setting speed is 1500 revs/min, and centrifugation stops after 25 minutes, after centrifugation, rich-titanium material density
Larger and color is black, and positioned at lower floor, remaining material density is smaller and color is grey, positioned at upper strata, by the upper and lower
Separation, lower floor is rich-titanium material, measures TiO in rich-titanium material2Content is 92.13%, the rate of recovery 82.15% of titanium.
Embodiment 7
It takes 450g ilmenite concentrates, between granularity is 150 ~ 200 μm, is put in Ball-stirring mill, weighs 450g oxalic acid, at 55 DEG C
Under be configured to solution, solution is poured into Ball-stirring mill, open Ball-stirring mill, rotating speed be 75 revs/min, the leaching at 55 DEG C
7.5 it is small when, stop stirring, filtering by filtrate crystallisation by cooling, recycles Citric acid crystal.Filter cake is pressed into filter cake：Water=1:3 matter
The mixture of filter cake and water is put into centrifuge, setting speed is 1500 revs/min, after centrifuging 25 minutes by amount than adding in water
Stop, after centrifugation, rich-titanium material density is larger and color is black, and positioned at lower floor, remaining material density is smaller and color is
Positioned at upper strata, the upper and lower are separated for grey, and lower floor is rich-titanium material, measure TiO in rich-titanium material2Content is 90.57%, titanium
The rate of recovery 80.77%.
Claims (6)
1. it is a kind of using ilmenite concentrate production rich-titanium material method, it is characterised in that whole process according to the following steps successively into
Row：（1）By ilmenite concentrate as in Ball-stirring mill, leaching agent is configured to the solution that concentration is 2.5% ~ 30% with water, then will
For solution as in Ball-stirring mill, for 1, than 0.1-2.5, leaching is stirred at room temperature in the weight ratio of ilmenite concentrate and leaching agent
When 5-10 is small；The leaching agent used is oxalic acid or citric acid；
（2）By the material filtering after leaching, filter cake and filtrate are obtained, filtrate is carried out fully according to the solubility curve of leaching agent
Cooling, makes excessive leaching agent crystallize into crystal in filtrate, is filtered again after crystallization, recycle excessive leaching agent；
（3）Filter cake is pressed into filter cake：Water=1:1 ~ 4 mass ratio adds in water, obtains slurry, slurry is centrifuged, centrifugation knot
Shu Hou, rich-titanium material density is larger and color is black, and positioned at lower floor, remaining material density is smaller and color is grey, positioned at upper
Layer, the upper and lower is separated, lower floor is rich-titanium material.
2. according to the method using ilmenite concentrate production rich-titanium material described in claim 1, it is characterised in that：The step
Suddenly（1）Described in the stirring slurry that uses of Ball-stirring mill for polytetrafluoroethylene (PTFE) material, agitated medium uses planetary native oxide
The ball of material.
3. according to the method using ilmenite concentrate production rich-titanium material described in claim 1, it is characterised in that：The step
Suddenly（1）In extraction temperature scope be 50 DEG C to 100 DEG C.
4. according to the method using ilmenite concentrate production rich-titanium material described in claim 1, it is characterised in that：The step
Suddenly（1）Described in Ball-stirring mill the range of speeds be 50 ~ 100 revs/min.
5. according to the method using ilmenite concentrate production rich-titanium material described in claim 1, it is characterised in that：The step
Suddenly（1）When the time range of middle leaching is 7.5-10 small.
6. according to the method using ilmenite concentrate production rich-titanium material described in claim 1, it is characterised in that：The richness
TiO in titanium material2Mass percentage be more than 90%, the rate of recovery be higher than 80%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AU4764796A (en) * | 1995-02-10 | 1996-08-27 | Bhp Minerals International, Inc. | Processing ilmenite ore to tio2 pigment |
| US7008602B2 (en) * | 2002-04-19 | 2006-03-07 | Millennium Inorganic Chemicals, Inc. | Beneficiation of titaniferous ore with sulfuric acid |
| GB0817021D0 (en) * | 2008-09-17 | 2008-10-22 | Univ Leeds | Process |
| CN101709374B (en) * | 2009-11-25 | 2011-05-11 | 中南大学 | Method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite |
| CN102352437B (en) * | 2011-09-15 | 2013-06-19 | 沙立林 | Method for treating hydrochloric acid leachate of ferrotitanium materials |
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